#------------------------------------------------------------------------------ #$Date: 2023-10-27 04:20:56 +0300 (Fri, 27 Oct 2023) $ #$Revision: 287134 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/75/7247590.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7247590 loop_ _publ_author_name 'Lim, Ae Ran' 'Kim, Sun Ha' _publ_section_title ; Processing on crystal growth, structure, thermal property, and nuclear magnetic resonance of organic--inorganic hybrid perovskite type [NH3(CH2)6NH3]ZnCl4 crystal ; _journal_issue 44 _journal_name_full 'RSC Advances' _journal_page_first 31027 _journal_page_last 31035 _journal_paper_doi 10.1039/D3RA05752F _journal_volume 13 _journal_year 2023 _chemical_formula_moiety 'C6 H18 N2, Cl4 Zn' _chemical_formula_sum 'C6 H18 Cl4 N2 Zn' _chemical_formula_weight 325.39 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc2h9btz _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-10-21 deposited with the CCDC. 2023-10-24 downloaded from the CCDC. ; _cell_angle_alpha 73.8420(10) _cell_angle_beta 87.9390(10) _cell_angle_gamma 85.6380(10) _cell_formula_units_Z 2 _cell_length_a 7.2972(3) _cell_length_b 10.1542(4) _cell_length_c 10.1812(3) _cell_measurement_reflns_used 8829 _cell_measurement_temperature 350(2) _cell_measurement_theta_max 24.33 _cell_measurement_theta_min 2.51 _cell_volume 722.41(5) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 350(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_unetI/netI 0.0177 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 27217 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.317 _diffrn_reflns_theta_min 2.093 _exptl_absorpt_coefficient_mu 2.406 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.496 _exptl_crystal_description BLOCK _exptl_crystal_F_000 332 _exptl_crystal_size_max 0.285 _exptl_crystal_size_mid 0.095 _exptl_crystal_size_min 0.090 _refine_diff_density_max 0.779 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.068 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 3595 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0446 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0951P)^2^+0.2857P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1405 _refine_ls_wR_factor_ref 0.1613 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2553 _reflns_number_total 3595 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra05752f1.cif _cod_data_source_block NH3CH26NH3ZnCl4_350K_a _cod_database_code 7247590 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.547 _shelx_estimated_absorpt_t_max 0.813 _shelx_res_file ; TITL NH3CH26NH3ZnCl4_350K_a.res in P-1 NH3CH26NH3ZnCl4_350K_a.res created by SHELXL-2018/3 at 14:38:28 on 23-Dec-2022 REM Old TITL NH3CH26NH3ZnCl4_350K in P-1 REM SHELXT solution in P-1 REM R1 0.138, Rweak 0.013, Alpha 0.032, Orientation as input REM Formula found by SHELXT: C6 Cl4 N2 Zn CELL 0.71073 7.2972 10.1542 10.1812 73.842 87.939 85.638 ZERR 2.000 0.0003 0.0004 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H CL N ZN UNIT 12 36 8 4 2 TEMP 77.000 SIZE 0.09 0.095 0.285 L.S. 10 BOND $H LIST 4 FMAP 2 PLAN 20 ACTA omit 0 0 1 WGHT 0.095100 0.285700 FVAR 1.06568 ZN1 5 0.262055 0.292666 0.442557 11.00000 0.05499 0.07198 = 0.07215 -0.01319 -0.00091 -0.00498 CL1 3 0.502763 0.207067 0.335923 11.00000 0.05587 0.09526 = 0.08358 -0.02772 0.00647 -0.00641 CL2 3 0.309825 0.210635 0.671509 11.00000 0.07847 0.07741 = 0.06949 -0.00809 0.00147 0.00071 CL3 3 0.241561 0.523384 0.378625 11.00000 0.12417 0.06683 = 0.08399 -0.00663 0.00171 -0.00277 CL4 3 0.007622 0.207408 0.384401 11.00000 0.05140 0.09077 = 0.11646 -0.03092 -0.00873 -0.00332 N1 4 0.722952 0.075508 0.638478 11.00000 0.07109 0.09221 = 0.07406 -0.01370 -0.01178 0.00392 AFIX 33 H1NA 2 0.770644 0.120612 0.558362 11.00000 -1.50000 H1NB 2 0.720429 -0.012971 0.642287 11.00000 -1.50000 H1NC 2 0.609118 0.110464 0.647455 11.00000 -1.50000 AFIX 0 N2 4 0.261163 0.513895 0.712624 11.00000 0.09536 0.07486 = 0.06949 -0.01699 -0.00688 -0.00458 AFIX 33 H2NA 2 0.180897 0.571630 0.657258 11.00000 -1.50000 H2NB 2 0.367169 0.552913 0.708486 11.00000 -1.50000 H2NC 2 0.279461 0.437064 0.686728 11.00000 -1.50000 AFIX 0 C1 1 0.835401 0.089298 0.748738 11.00000 0.11489 0.10083 = 0.09404 -0.02250 -0.02337 -0.01848 AFIX 23 H1A 2 0.959717 0.053593 0.735506 11.00000 -1.20000 H1AB 2 0.839974 0.186378 0.741065 11.00000 -1.20000 AFIX 0 C2 1 0.778357 0.024890 0.878376 11.00000 0.20460 0.18362 = 0.10400 0.00637 -0.02298 -0.06997 AFIX 23 H2A 2 0.770223 -0.071915 0.886239 11.00000 -1.20000 H2AB 2 0.656099 0.062869 0.893865 11.00000 -1.20000 AFIX 0 C3 1 0.909842 0.039310 0.993471 11.00000 0.18680 0.22792 = 0.09914 -0.03617 -0.01458 -0.05835 AFIX 23 H3A 2 0.931253 0.135784 0.976436 11.00000 -1.20000 H3AB 2 0.845300 0.011469 1.080701 11.00000 -1.20000 AFIX 0 C4 1 0.188619 0.481077 0.853308 11.00000 0.09674 0.15307 = 0.08004 -0.01231 0.00025 -0.02615 AFIX 23 H4A 2 0.165655 0.566207 0.878653 11.00000 -1.20000 H4AB 2 0.071295 0.441572 0.855245 11.00000 -1.20000 AFIX 0 C5 1 0.303327 0.388732 0.954503 11.00000 0.18433 0.18277 = 0.08746 -0.01903 0.01085 -0.05662 AFIX 23 H5A 2 0.324115 0.302685 0.930630 11.00000 -1.20000 H5AB 2 0.237981 0.369664 1.041699 11.00000 -1.20000 AFIX 0 C6 1 0.500891 0.443674 0.973021 11.00000 0.13473 0.20003 = 0.07659 -0.02124 0.00373 -0.02523 AFIX 23 H6A 2 0.574641 0.368252 1.031949 11.00000 -1.20000 H6AB 2 0.562291 0.467965 0.884318 11.00000 -1.20000 AFIX 0 HKLF 4 REM NH3CH26NH3ZnCl4_350K_a.res in P-1 REM wR2 = 0.161275, GooF = S = 1.02138, Restrained GooF = 1.02138 for all data REM R1 = 0.044594 for 2553 Fo > 4sig(Fo) and 0.065593 for all 3595 data REM 118 parameters refined using 0 restraints END WGHT 0.0833 0.3491 REM Highest difference peak 0.779, deepest hole -0.430, 1-sigma level 0.068 Q1 1 0.2710 0.5420 0.9438 11.00000 0.05 0.78 Q2 1 0.9392 -0.0081 0.8253 11.00000 0.05 0.72 Q3 1 0.4428 0.3645 0.9582 11.00000 0.05 0.39 Q4 1 0.7189 0.0875 0.7909 11.00000 0.05 0.35 Q5 1 0.3273 0.5333 0.4112 11.00000 0.05 0.31 Q6 1 0.0356 0.1779 0.4704 11.00000 0.05 0.31 Q7 1 0.4375 0.2164 0.2738 11.00000 0.05 0.30 Q8 1 0.9780 -0.0209 1.0650 11.00000 0.05 0.27 Q9 1 0.8390 0.1231 0.8603 11.00000 0.05 0.27 Q10 1 0.4846 0.1352 0.3897 11.00000 0.05 0.23 Q11 1 0.5453 0.4575 1.0571 11.00000 0.05 0.23 Q12 1 0.2469 0.5063 0.3105 11.00000 0.05 0.22 Q13 1 0.1502 0.5347 0.4186 11.00000 0.05 0.22 Q14 1 0.7837 0.0967 0.9959 11.00000 0.05 0.21 Q15 1 0.4087 0.2479 0.6820 11.00000 0.05 0.19 Q16 1 0.2487 0.3065 0.3627 11.00000 0.05 0.19 Q17 1 0.2490 0.4324 0.3977 11.00000 0.05 0.19 Q18 1 0.0060 0.3015 0.3391 11.00000 0.05 0.18 Q19 1 0.2622 0.2157 0.5846 11.00000 0.05 0.17 Q20 1 0.4672 0.0831 0.3242 11.00000 0.05 0.16 ; _shelx_res_checksum 31140 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.26205(5) 0.29267(4) 0.44256(4) 0.06770(19) Uani 1 1 d . . . . . Cl1 Cl 0.50276(13) 0.20707(12) 0.33592(11) 0.0778(3) Uani 1 1 d . . . . . Cl2 Cl 0.30983(15) 0.21063(11) 0.67151(10) 0.0780(3) Uani 1 1 d . . . . . Cl3 Cl 0.2416(2) 0.52338(11) 0.37862(12) 0.0948(4) Uani 1 1 d . . . . . Cl4 Cl 0.00762(13) 0.20741(12) 0.38440(13) 0.0857(3) Uani 1 1 d . . . . . N1 N 0.7230(5) 0.0755(4) 0.6385(4) 0.0812(9) Uani 1 1 d . . . . . H1NA H 0.770644 0.120612 0.558362 0.122 Uiso 1 1 calc R U . . . H1NB H 0.720429 -0.012971 0.642287 0.122 Uiso 1 1 calc R U . . . H1NC H 0.609118 0.110464 0.647455 0.122 Uiso 1 1 calc R U . . . N2 N 0.2612(6) 0.5139(4) 0.7126(3) 0.0804(9) Uani 1 1 d . . . . . H2NA H 0.180897 0.571630 0.657258 0.121 Uiso 1 1 calc R U . . . H2NB H 0.367169 0.552913 0.708486 0.121 Uiso 1 1 calc R U . . . H2NC H 0.279461 0.437064 0.686728 0.121 Uiso 1 1 calc R U . . . C1 C 0.8354(9) 0.0893(6) 0.7487(5) 0.1030(15) Uani 1 1 d . . . . . H1A H 0.959717 0.053593 0.735506 0.124 Uiso 1 1 calc R U . . . H1AB H 0.839974 0.186378 0.741065 0.124 Uiso 1 1 calc R U . . . C2 C 0.7784(15) 0.0249(10) 0.8784(7) 0.170(4) Uani 1 1 d . . . . . H2A H 0.770223 -0.071915 0.886239 0.204 Uiso 1 1 calc R U . . . H2AB H 0.656099 0.062869 0.893865 0.204 Uiso 1 1 calc R U . . . C3 C 0.9098(13) 0.0393(12) 0.9935(9) 0.170(4) Uani 1 1 d . . . . . H3A H 0.931253 0.135784 0.976436 0.205 Uiso 1 1 calc R U . . . H3AB H 0.845300 0.011469 1.080701 0.205 Uiso 1 1 calc R U . . . C4 C 0.1886(8) 0.4811(7) 0.8533(5) 0.1131(18) Uani 1 1 d . . . . . H4A H 0.165655 0.566207 0.878653 0.136 Uiso 1 1 calc R U . . . H4AB H 0.071295 0.441572 0.855245 0.136 Uiso 1 1 calc R U . . . C5 C 0.3033(13) 0.3887(10) 0.9545(7) 0.153(3) Uani 1 1 d . . . . . H5A H 0.324115 0.302685 0.930630 0.184 Uiso 1 1 calc R U . . . H5AB H 0.237981 0.369664 1.041699 0.184 Uiso 1 1 calc R U . . . C6 C 0.5009(11) 0.4437(9) 0.9730(6) 0.140(3) Uani 1 1 d . . . . . H6A H 0.574641 0.368252 1.031949 0.168 Uiso 1 1 calc R U . . . H6AB H 0.562291 0.467965 0.884318 0.168 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0550(3) 0.0720(3) 0.0722(3) -0.0132(2) -0.00091(19) -0.00498(19) Cl1 0.0559(5) 0.0953(7) 0.0836(6) -0.0277(5) 0.0065(4) -0.0064(4) Cl2 0.0785(6) 0.0774(6) 0.0695(6) -0.0081(4) 0.0015(4) 0.0007(5) Cl3 0.1242(10) 0.0668(6) 0.0840(7) -0.0066(5) 0.0017(6) -0.0028(6) Cl4 0.0514(5) 0.0908(7) 0.1165(8) -0.0309(6) -0.0087(5) -0.0033(4) N1 0.071(2) 0.092(2) 0.074(2) -0.0137(17) -0.0118(16) 0.0039(17) N2 0.095(3) 0.075(2) 0.0695(19) -0.0170(16) -0.0069(17) -0.0046(18) C1 0.115(4) 0.101(3) 0.094(3) -0.022(3) -0.023(3) -0.018(3) C2 0.205(10) 0.184(8) 0.104(5) 0.006(5) -0.023(5) -0.070(7) C3 0.187(9) 0.228(11) 0.099(4) -0.036(6) -0.015(6) -0.058(8) C4 0.097(4) 0.153(5) 0.080(3) -0.012(3) 0.000(3) -0.026(4) C5 0.184(8) 0.183(7) 0.087(4) -0.019(4) 0.011(4) -0.057(6) C6 0.135(6) 0.200(9) 0.077(4) -0.021(4) 0.004(4) -0.025(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl3 Zn1 Cl4 111.51(5) . . ? Cl3 Zn1 Cl1 111.30(5) . . ? Cl4 Zn1 Cl1 105.94(4) . . ? Cl3 Zn1 Cl2 110.61(4) . . ? Cl4 Zn1 Cl2 110.37(5) . . ? Cl1 Zn1 Cl2 106.92(4) . . ? C1 N1 H1NA 109.5 . . ? C1 N1 H1NB 109.5 . . ? H1NA N1 H1NB 109.5 . . ? C1 N1 H1NC 109.5 . . ? H1NA N1 H1NC 109.5 . . ? H1NB N1 H1NC 109.5 . . ? C4 N2 H2NA 109.5 . . ? C4 N2 H2NB 109.5 . . ? H2NA N2 H2NB 109.5 . . ? C4 N2 H2NC 109.5 . . ? H2NA N2 H2NC 109.5 . . ? H2NB N2 H2NC 109.5 . . ? C2 C1 N1 116.0(6) . . ? C2 C1 H1A 108.3 . . ? N1 C1 H1A 108.3 . . ? C2 C1 H1AB 108.3 . . ? N1 C1 H1AB 108.3 . . ? H1A C1 H1AB 107.4 . . ? C1 C2 C3 113.6(8) . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2AB 108.8 . . ? C3 C2 H2AB 108.8 . . ? H2A C2 H2AB 107.7 . . ? C3 C3 C2 117.0(10) 2_757 . ? C3 C3 H3A 108.0 2_757 . ? C2 C3 H3A 108.0 . . ? C3 C3 H3AB 108.0 2_757 . ? C2 C3 H3AB 108.0 . . ? H3A C3 H3AB 107.3 . . ? C5 C4 N2 115.9(6) . . ? C5 C4 H4A 108.3 . . ? N2 C4 H4A 108.3 . . ? C5 C4 H4AB 108.3 . . ? N2 C4 H4AB 108.3 . . ? H4A C4 H4AB 107.4 . . ? C4 C5 C6 115.0(7) . . ? C4 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? C4 C5 H5AB 108.5 . . ? C6 C5 H5AB 108.5 . . ? H5A C5 H5AB 107.5 . . ? C6 C6 C5 116.8(9) 2_667 . ? C6 C6 H6A 108.1 2_667 . ? C5 C6 H6A 108.1 . . ? C6 C6 H6AB 108.1 2_667 . ? C5 C6 H6AB 108.1 . . ? H6A C6 H6AB 107.3 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 Cl3 2.2449(12) . ? Zn1 Cl4 2.2707(11) . ? Zn1 Cl1 2.2749(10) . ? Zn1 Cl2 2.2765(11) . ? N1 C1 1.458(6) . ? N1 H1NA 0.8900 . ? N1 H1NB 0.8900 . ? N1 H1NC 0.8900 . ? N2 C4 1.466(6) . ? N2 H2NA 0.8900 . ? N2 H2NB 0.8900 . ? N2 H2NC 0.8900 . ? C1 C2 1.365(9) . ? C1 H1A 0.9700 . ? C1 H1AB 0.9700 . ? C2 C3 1.585(11) . ? C2 H2A 0.9700 . ? C2 H2AB 0.9700 . ? C3 C3 1.476(19) 2_757 ? C3 H3A 0.9700 . ? C3 H3AB 0.9700 . ? C4 C5 1.431(10) . ? C4 H4A 0.9700 . ? C4 H4AB 0.9700 . ? C5 C6 1.620(12) . ? C5 H5A 0.9700 . ? C5 H5AB 0.9700 . ? C6 C6 1.399(15) 2_667 ? C6 H6A 0.9700 . ? C6 H6AB 0.9700 . ?